Impurities, either synthetic or degradative, found in drug products or drug dosage forms have been associated with adverse effects including increased toxicity, decreased efficacy of the active drug, and other undesirable side effects. Such impurities, once identified, are reduced to the lowest possible levels to lessen the risk of adverse events. 3,4-Diaminopyridine is a central nervous system drug used in the treatment of Lambert/Eaton Myasthenic Syndrome (LEMS) and other rare muscle diseases. A great need exists for the ability to ascertain whether amounts of 3,4-diaminopyridine have degraded. It is greatly desired to be able to quantitate the amount of degradation present in a 3,4-diaminopyridine sample. There also exists a need for highly sensitive means of detecting impurities in a sample of 3,4-diaminopyridine, determining the purity of a sample of 3,4-diaminopyridine, and quantitating the amount of impurities present in a 3,4-diaminopyridine sample.